The present invention provides synergistic composition of bioactive amounts of Profenofos at least one insecticide of neonicotinoid class selected from Clothianidin, Thiamethoxam and Imidacloprid and at least one more insecticide selected from Bifenthrin, Fipronil, Fenpyroximate, Flonicamid and Tolfenpyrad with one or more inactive excipient.
"Bioactive amounts” as mentioned herein means that amount which, when applied treatment of crops, is sufficient to effect such treatment.

Advantageous invention relates to a synergistic composition of bioactive amounts of Profenofos at least one insecticide of neonicotinoid class selected from Clothianidin, Thiamethoxam and Imidacloprid and at least one more insecticide selected from Bifenthrin, Fipronil, Fenpyroximate, Flonicamid and Tolfenpyrad with one or more inactive excipient.

Further the concentration of active ingredients is present in the ranges as mentioned in below table;

% of components varies from
Active 1 Active 2 Active 3
Profenofos Clothianidin
Thiamethoxam
Imidacloprid Bifenthrin
Fipronil
Fenpyroximate
Flonicamid
Tolfenpyrad
% concentration 0.1 to 50% 0.1 to 25% 0.1 to 25%

As per one embodiment, the composition of present invention is Effective for protection of plants, agricultural and horticultural crops like Genetically Modified Organism (GMO) and non GMO Plant of Cotton (Gossypium spp.), Jute (Corchorus oliotorus), Paddy (Oryza sativa), Wheat (Triticum aestavum), Barley (Hordeum vulgare), Maize (Zea mays), Sorghum (Sorghum bicolor), Ragi (Eleusine coracana), Pearl millet (Pennisetum glaucum), Sugarcane (Saccharum officinarum) , Sugarbeet (Beta vulgaris), Soybean (Glycine max), Peanut (Arachis hypogaea), Sunflower (Helianthus annuus) , Mustard (Brassica juncea), Rape seed (Brassica napus), Linseed (Linum usitatissimum), Sesame (Sesamum indicum), Castor (Ricinus communis), Green gram (Vigna radiate), Black gram (Vigna mungo), Chickpea (Cicer aritinum), Cowpea (Vigna unguiculata), Redgram (Cajanus cajan), Frenchbean (Phaseolus vulgaris), Indian bean (Lablab purpureus), Horse gram (Macrotyloma uniflorum), Field pea (Pisum sativum), Cluster bean (Cyamopsis tetragonoloba), Lentils (Lens culinaris), Brinjal (Solanum melongena), Cabbage (Brassica oleracea var. capitata), Cauliflower (Brassica oleracea var. botrytis), Okra (Abelmoschus esculentus) , Onion (Allium cepa L.), Tomato (Solanum lycopersicun) , Potato (Solanum tuberosum) , Sweet potato (Ipomoea batatas), Chilly (Capsicum annum), Garlic (Allium sativum), Cucumber (Cucumis sativus) and Melons (Cucumis melo), Radish (Raphanus sativus), Carrot (Dacus carota subsp. sativus), Turnip (Brassica rapa subsp rapa), Apple (Melus domestica), Banana (Musa spp.), Citrus groups (Citrus spp.), Grape (Vitis vinifera), Guava (Psidium guajava), Litchi (Litchi chinensis), Mango (Mangifera indica), Papaya (Carica papaya), Pineapple (Ananas comosus), Pomegranate (Punica granatum) , Sapota (Manilkara zapota), Tea (Camellia sinensis), Coffea (Coffea Arabica), Turmeric (Curcuma longa), Ginger (Zingiber officinale), Cumin (Cuminum cyminum), Fenugreek (Trigonella foenum-graecum), Fennel (Foeniculum vulgare), Coriander (Coriandrum sativum), Ajwain (Trachyspermum ammi), Psyllium (Plantago ovate), Black Pepper (Piper nigrum), Stevia (Stevia rebaudiana), Safed musli (Chlorophytum tuberosum), Drum stick (Moringa oleifera), Coconut (Coco nucifera), Mentha ( Mentha spp.), Rose (Rosa spp.), Jasmine (Jasminum spp.), Marigold ( Tagetes spp.), Common daisy (Bellis perennis), Dahlia (Dahlia hortnesis).

The composition of the present invention can be used to control or to manage the insects-pests belongs to the order Hemiptera, for example, various species of Mealybug (Paracoccus marginatus, Phenococcus aceris, Phenacoccus solenopsis, Phenacoccus citri, Planococcus citri, Maconellicoccus hirsutus, Pseudococcus hirsutus, Saccharicoccus sacchari etc.) infesting cotton, sugarcane, grape, papaya, pomegranate, apple, citrus,custard apple, banana, ornamental plant etc., Scale insects (Aonidiella auruntii, Ceroplastes sinensis, Saissetia oleae etc) infesting citrus, apple, grape and other horticultural crops and forest trees, bean aphid (Aphis fabae), black citrus aphid (Toxoptera aurantii), cabbage aphid (Brevicoryne brassicae, Lipaphis erysimi), corn leaf aphid (Rhopalosiphum maidis), cotton aphid (Aphis gossypii), cotton leaf hoppers (Amrasca biguttula biguttula), cotton stainer (Dysdercus suturellus), cotton whitefly (Bemisia tabaci), cowpea aphid (Aphis crassivora), grain aphid (Sitobion avenae), safflower aphid (Uroleucon spp.), green peach aphid (Myzus persicae), greenhouse whitefly (Trialeurodes vaporariorum)spp., pea aphid (Acyrthosiphon pisum), potato aphid (Myzus persicae), potato leaf hopper (Empoasca fabae), rice leafhopper (Nephotettix nigropictus), rice brown plant hopper (Nilaparvata lugen), tarnished plant bug (Lygus lineolaris), wooly apple aphid (Eriosoma lanigerum), tea mosquito bug (Helopeltis theivora), order Lepidoptera, army worm (Mythimna unipuncta), asiatic rice borer (Chilo suppressalis), maize stem borer (Chilo partellus), bean pod borer (Maruca vitrata), beet armyworm (Spodoptera exigua), black cutworm (Agrotis ipsilon), American bollworm (Helicoverpa armigera),cabbage looper (Trichoplusia ni), codling moth (Cydia pomonella), croton caterpillar (Achea janata), diamond backmoth (Plutella xylostella), cabbage worm (Pieris rapae), pink bollworm (Pectinophora gossypiella), sugarcane borer (Diatraea saccharalis), tobacco budworm (Heliothis virescens), tomato fruitworm (Helicoverpa zea), velvet bean caterpillar (Anticarsia gemmatalis), yellow stem borer (SCirpophaga incertulas), spotted bollworm (Earias vittella), rice leaffolder (Cnaphalocrocis medinalis), pink stem borer (Sesamia spp.), tobacco leafeating caterpillar (Spodoptera litura), tea looper (Biston supressaria) ; from the order Coleoptera, for example, apple twig borer (Amphicerus spp.), corn root worm (Diabrotica virgifera), cucumber beetle (diabrotica balteata), boll weevil (Anthonomus grandis), grape flea beetle (Altica chalybea), grape root worm (Fidia viticola), grape trunk borer (Clytoleptus albofasciatus), radish flea beetle (Phyllotreta armoraciae), maize weevil (Sitophilus zeamais), northern corn rootworm (Diabrotica barberi), rice water weevil (Lissorhoptrus oryzophilus; from the order Orthoptera, for example, Gryllotalpa spp., Locusta spp., and Schistocerca is spp.; from the order Thysanoptera, for example, Anaphothrips obscurus, Baliothrips biformis, Drepanothrips reuteri, Enneothrips flavens, Frankliniella spp., Heliothripsspp., Hercinothrips femoralis, Rhipiphorothrips cruentatus, Scirtothrips spp., Taeniothrips cardamomi, Frankliniella spp., Thrips palmi, Thrips tabaci and Scirtothrips dorsalis; from the order Heteroptera, for example, Dysdercus spp., Leptocorisa spp., from the order Hymenoptera, for example, Solenopsis spp. ; from the order Diptera, for example, Atherigona soccata, Atherigona orientalis, Dacus spp., Liriomyza spp., Melanagromyza spp., from the order Acarina, for example, Aceria mangiferae, Brevipalpus spp., Eriophyes spp., Oligonychus mangiferus, Oligonychus punicae, Panonychus citri, Panonychus ulmi, Polyphagotarsonemus latus, Tarsonemus spp., Tetranychus urticae, Tetranychus cinnabarinus.

Composition of the present invention can be in any of the form described above.

The synergistic composition of bioactive amounts of Profenofos at least one insecticide of neonicotinoid class and at least one more insecticide further comprises inactive excipients including but not limited to dispersant, anti-freezing agent, anti-foam agent,wetting agent, suspension aid,anti-microbial agent, thickener, quick coating agent or sticking agents (also referred to as “stickers” or “binders”) and buffering agent.

A dispersant is a substance which adsorbs onto the surface of particles and helps to preserve the state of dispersion of the particles and prevents them from re-aggregating. Dispersants are added to agrochemical compositions to facilitate dispersion and suspension during manufacture, and to ensure the particles re-disperse into water in a spray tank. They are widely used in wettable powders, suspension concentrates and water-dispersible granules. Surfactants that are used as dispersants have the ability to adsorb strongly onto a particle surface and provide a charged or steric barrier to re-aggregation of particles. The most commonly used surfactants are anionic, non-ionic, or mixtures of the two types. For wettable powder compositions, the most common dispersants are sodium lignosulphonates. For suspension concentrates, very good adsorption and stabilization are obtained using polyelectrolytes, such as sodium naphthalene sulphonate formaldehyde condensates. Tristyrylphenolethoxylate phosphate esters are also used. Nonionics such as alkylarylethylene oxide condensates and EO-PO block copolymers are sometimes combined with anionics as dispersants for suspension concentrates. In recent years, new types of very high molecular weight polymeric surfactants have been developed as dispersants. These have very long hydrophobic ‘backbones’ and a large number of ethylene oxide chains forming the ‘teeth’ of a ‘comb’ surfactant. These high molecular weight polymers can give very good long-term stability to suspension concentrates because the hydrophobic backbones have many anchoring points onto the particle surfaces. Examples of dispersants used herein include but not limited to sodium lignosulphonates; sodium naphthalene sulphonate formaldehyde condensates; tristyrylphenolethoxylate phosphate esters; aliphatic alcohol ethoxylates; alky ethoxylates; EO-PO block copolymers; and graft copolymers or mixtures thereof.

Anti-freezing agent as used herein can be selected from the group consisting of polyethylene glycols, methoxypolyethylene glycols, polypropylene glycols, polybutylene glycols, glycerin and ethylene glycol.

Water-based compositions often cause foam during mixing operations in production. In order to reduce the tendency to foam, anti-foam agents are often added either during the production stage or before filling into bottles. Generally, there are two types of anti-foam agents, namely silicones and non-silicones. Silicones are usually aqueous emulsions of dimethyl polysiloxane while the non-silicone anti-foam agents are water-insoluble oils, such as octanol and nonanol, or silica. In both cases, the function of the anti-foam agent is to displace the surfactant from the air-water interface.

A wetting agent is a substance that when added to a liquid increases the spreading or penetration power of the liquid by reducing the interfacial tension between the liquid and the surface on which it is spreading. Wetting agents are used for two main functions in agrochemical compositions: during processing and manufacture to increase the rate of wetting of powders in water to make concentrates for soluble liquids or suspension concentrates; and during mixing of a product with water in a spray tank or other vessel to reduce the wetting time of wettable powders and to improve the penetration of water into water-dispersible granules. Examples of wetting agents used in wettable powder, suspension concentrate, and water-dispersible granule compositions include but not limited to sodium lauryl sulphate; sodium dioctylsulphosuccinate; alkyl phenol ethoxylates; and aliphatic alcohol ethoxylates or mixtures thereof.

Suspension aid in the present description denotes a natural or synthetic, organic or inorganic material with which the active substance is combined in order to facilitate its application to the plant, to the seeds or to the soil. This carrier is hence generally inert, and it must be agriculturally acceptable, in particular to the plant being treated. The carrier may be solid (clays, natural or synthetic silicates, silica, resins, waxes, solid fertilizers, and the like or mixtures thereof) or liquid (water, alcohols, ketones, petroleum fractions, aromatic or paraffinic hydrocarbons, chlorinated hydrocarbons, liquefied gases, and the like or mixtures thereof).

Biocides / Microorganisms cause spoilage of formulated products. Therefore anti-microbial agents are used to eliminate or reduce their effect. Examples of such agents include, but are not limited to: propionic acid and its sodium salt; sorbic acid and its sodium or potassium salts; benzoic acid and its sodium salt; p-hydroxy benzoic acid sodium salt; methyl p-hydroxy benzoate; and biocide such as sodium benzoate, 1,2-benzisothiazoline-3-one, 2-methyl-4-isothiazolin-3-one, 5-chloro-2-methyl-4-isothiazolin-3-one, potassium sorbate, parahydroxy benzoates or mixtures thereof.

Thickeners or gelling agents are used mainly in the composition of suspension concentrates, emulsions and suspoemulsions to modify the rheology or flow properties of the liquid and to prevent separation and settling of the dispersed particles or droplets. Thickening, gelling, and anti-settling agents generally fall into two categories, namely water-insoluble particulates and water-soluble polymers. It is possible to produce suspension concentrate compositions using clays and silicas. Examples of these types of materials, include, but are limited to, montmorillonite, e.g. bentonite; magnesium aluminum silicate; and attapulgite. Water-soluble polysaccharides have been used as thickening-gelling agents for many years. The types of polysaccharides most commonly used are natural extracts of seeds and seaweeds are synthetic derivatives of cellulose or mixtures thereof. Examples of these types of materials include, but are not limited to, guar gum; locust bean gum; carrageenam; xanthan gum; alginates; methyl cellulose; sodium carboxymethyl cellulose (SCMC); hydroxyethyl cellulose (HEC) or mixtures thereof. Other types of anti-settling agents are based on modified starches, polyacrylates, polyvinyl alcohol and polyethylene oxide or mixtures.

The quick coating agentcan be a conventionally available sticker, for example polyesters, polyamides, poly- carbonates, polyurea and polyurethanes, acrylate polymers and copolymers, styrene copolymers, butadiene copolymers, polysaccharides such as starch and cellulose derivatives, vinylalcohol, vinylacetate and vinylpyrrolidone polymers and copolymers, polyethers, epoxy, phenolic and melamine resins, polyolefins and define copolymersand mixtures thereof. Examples of preferred polymers are acrylate polymers such as poly(methacrylate), poly(ethyl methacrylate), poly(methylmethacrylate), acrylate copoylmers and styrene-acrylic copolymers as defined herein below, poly(styrene-co maleic anhydride), cellulosic polymers such as ethyl cellulose, cellulose acetate, cellulose acetatebutyrate, acetylated mono, di, and triglycerides, poly(vinylpyrrolidone), vinyl acetate polymers and copolymers, poly(alkylene glycol), styrene butadiene copolymers, poly(orthoesters), alkyd resins, and mixtures of two or more of these. Polymers that are biodegradable are also useful in the present invention. As used herein, a polymer is biodegradable if is not water soluble, but is degraded over a period of several weeks when placed in an application environment. Examples of biodegradable polymers that are useful in the present invention include biodegradable polyesters, starch, polylactic acid starch blends, polylactic acid, poly(lactic acid-glycolic acid) copolymers, polydioxanone, cellulose esters, ethyl cellulose, cellulose acetate butyrate, starch esters, starch esteraliphatic polyester blends, modified corn starch, polycaprolactone, poly(namylmethacrylate), wood rosin, polyanhydrides, polyvinylalcohol, polyhydroxybutyratevalerate, biodegradable aliphatic polyesters, and polyhydroxybutyrate or mixtures thereof.

Buffering agent as used herein is selected from group consisting of calcium hydroxyapatite, PottasiumDihydrogen Phosphate, Sodium Hydroxide, carbonated apatite, calcium carbonate, sodium bicarbonate, tricalcium phosphate, calcium phosphates, carbonated calcium phosphates, amine monomers, lactate dehydrogenase and magnesium hydroxide.

The solvent for the composition of the present invention may include water, water-soluble alcohols and dihydroxy alcohol ethers. The water-soluble alcohol which can be used in the present invention may be lower alcohols or water-soluble macromolecular alcohols. The term "lower alcohol", as used herein, represents an alcohol having 1-4 carbon atoms, such as methanol, ethanol, n-propanol, isopropanol, n-butanol, tert-butanol, etc. Macromolecular alcohol is not limited, as long as it may be dissolved in water in a suitable amount range, e.g., polyethylene glycol, sorbitol, glucitol, etc. The examples of suitable dihydroxy alcohol ethers used in the present invention may be dihydroxy alcohol alkyl ethers or dihydroxy alcohol aryl ethers. The examples of dihydroxy alcohol alkyl ether include ethylene glycol methyl ether, diethylene glycol methyl ether, propylene glycol methyl ether, dipropylene glycol methyl ether, ethylene glycol ethyl ether, diethylene glycol ethyl ether, propylene glycol ethyl ether, dipropylene glycol ethyl ether, etc. The examples of dihydroxy alcohol aryl ethers include ethylene glycol phenyl ether, diethylene glycol phenyl ether, propylene glycol phenyl ether, dipropylene glycol phenyl ether, and the like. Any of the above mentioned solvent can be used either alone or in combination thereof.

EXAMPLES

Example 1: Profenofos 30% + clothianidin 7.5% + Bifenthrin 7.5% EC
Ingredient Percentage (w/w)
Profenofos Technical A.I. 30
Clothianidin Technical A.I. 7.5
Bifenthrin Technical A.I. 7.5
N-Methyl-2-pyrrolidone 5
Polyaryl phenol ethoxylate (40-70%) & calcium dodecyl benzene solphonate (20-40%) 5.9
Polyaryl phenol ethoxylate(20-40%) & calcium dodecyl benzene solphonate (40-60%) 4.1
Trisiloxane Ethoxylate 2
Mixture of heavy aromatic hydrocarbons QS
TOTAL 100.0

Procedure:
Step 1 Charge required quantity of solvent and then mix the technical into this solvent until completely soluble
Step 2 Now add surfactants dose as per screening ration
Step 3 Now add remaining solvent to this mixture
Step 4 Final product is sent for QC approval.
Step 5 After approval material is packed in required pack sizes.

Storage stability study
Parameters Specification
(In house) Initial Stability (for 14 days)
At 54±20C At 0±20C
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.15 30.11 30.15
Clothianidin content (% w/w) 7.125 to 8.25 7.60 7.58 7.59
Bifenthrin Content (% w/w) 7.125 to 8.25 7.62 7.59 7.60
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.02 7.01 7.03
Flash point Above 24.5 degree celcius 43 43 43
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies

Room temperature storage data
Parameters Specification
(In house) Study Duration
1 month 6 month 12 month
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.15 30.15 30.14
Clothianidin content (% w/w) 7.125 to 8.25 7.60 7.60 7.59
Bifenthrin Content (% w/w) 7.125 to 8.25 7.62 7.62 7.61
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.02 7.02 7.01
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies
Flash point Above 24.5 degree celcius 43 43 43

Example 2: Profenofos 30% + Clothianidin 7.5% + Tolfenpyrad 7.5% EC
Ingredient Percentage (w/w)
Profenofos Technical A.I. 30
Clothianidin Technical A.I. 7.5
Tolfenpyrad Technical A.I. 7.5
N-Methyl-2-pyrrolidone 5
Polyaryl phenol ethoxylate (40-70%) & calcium dodecyl benzene solphonate (20-40%) 5.8
Polyaryl phenol ethoxylate (20-40%) & calcium dodecyl benzene solphonate (40-60%) 4.2
Trisiloxane Ethoxylate 2
Mixture of heavy aromatic hydrocarbons QS
TOTAL 100.0

Procedure: As per Example 1

Storage stability study
Parameters Specification
(In house) Initial Stability (for 14 days)
At 54±20C At 0±20C
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.20 30.14 30.18
Clothianidin content (% w/w) 7.125 to 8.25 7.63 7.58 7.61
Tolfenpyrad Content (% w/w) 7.125 to 8.25 7.59 7.55 7.59
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.07 7.03 7.06
Flash point Above 24.5 degree celcius 43 43 43
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies

Room temperature storage data
Parameters Specification
(In house) Study Duration
1 month 6 month 12 month
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.20 30.19 30.17
Clothianidin content (% w/w) 7.125 to 8.25 7.62 7.62 7.61
Tolfenpyrad Content (% w/w) 7.125 to 8.25 7.59 7.58 7.58
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.07 7.07 7.05
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies
Flash point Above 24.5 degree celcius 43 43 43

Example 3: Profenofos 30% + Thiamethoxam 7.5% + Bifenthrin 7.5% EC
Ingredient Percentage (w/w)
Profenofos Technical A.I. 30
ThiamethoxamTechnical A.I. 7.5
Bifenthrin Technical A.I. 7.5
N-Methyl-2-pyrrolidone 5
Polyaryl phenol ethoxylate (40-70%) & calcium dodecyl benzene solphonate (20-40%) 5.9
Polyaryl phenol ethoxylate (20-40%) & calcium dodecyl benzene solphonate (40-60%) 4.1
Trisiloxane Ethoxylate 2
Mixture of heavy aromatic hydrocarbons QS
TOTAL 100.0

Procedure: As per Example 1

Storage stability study
Parameters Specification
(In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.25 30.16 30.22
Thiamethoxam content (% w/w) 7.125 to 8.25 7.58 7.51 7.55
Bifenthrin Content (% w/w) 7.125 to 8.25 7.62 7.53 7.60
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.08 7.02 7.08
Flash point Above 24.5 degree celcius 43 43 43
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 month
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.24 30.23 30.22
Thiamethoxam content (% w/w) 7.125 to 8.25 7.57 7.57 7.55
Bifenthrin Content (% w/w) 7.125 to 8.25 7.62 7.61 7.59
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.08 7.06 7.05
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies
Flash point Above 24.5 degree celcius 43 43 43

Example 4: Profenofos 30% + Thiamethoxam 7.5% + Tolfenpyrad 7.5% EC
Ingredient Percentage (w/w)
Profenofos Technical A.I. 30
ThiamethoxamTechnical A.I. 7.5
Tolfenpyrad Technical A.I. 7.5
N-Methyl-2-pyrrolidone 5
Polyaryl phenol ethoxylate (40-70%) & calcium dodecyl benzene solphonate (20-40%) 5.5
Polyaryl phenol ethoxylate (20-40%) & calcium dodecyl benzene solphonate (40-60%) 4.5
Trisiloxane Ethoxylate 2
Mixture of heavy aromatic hydrocarbons QS
TOTAL 100.0

Procedure: As per Example 1

Storage stability study
Parameters Specification
(In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.3 30.12 30.28
Thiamethoxam content (% w/w) 7.125 to 8.25 7.55 7.49 7.55
Tolfenpyrad Content (% w/w) 7.125 to 8.25 7.65 7.59 7.64
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 6.97 6.99 6.96
Flash point Above 24.5 degree celcius 43 43 43
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 month
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.3 50.16 50.14
Thiamethoxam content (% w/w) 7.125 to 8.25 7.55 7.54 7.54
Tolfenpyrad Content (% w/w) 7.125 to 8.25 7.65 7.64 7.64
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 6.97 6.97 6.99
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies
Flash point Above 24.5 degree celcius 43 43 43

Example 5: Profenofos 30% + clothianidin 7.5% + Fenpyroximate 5% EC
Ingredient Percentage (w/w)
Profenofos Technical A.I. 30
Clothianidin Technical A.I. 7.5
Fenpyroximate Technical A.I. 5
N-Methyl-2-pyrrolidone 6
Polyaryl phenol ethoxylate (40-70%) & calcium dodecyl benzene solphonate (20-40%) 6
Polyaryl phenol ethoxylate (20-40%) & calcium dodecyl benzene solphonate (40-60%) 4
Trisiloxane Ethoxylate 2
Mixture of heavy aromatic hydrocarbons QS
TOTAL 100.0

Procedure: As per Example 1
Storage stability study
Parameters Specification
(In house) Initial Stability (for 14 days)
At 54±20C At 0±20C
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.60 30.55 30.6
Clothianidin content (% w/w) 7.125 to 8.25 7.55 7.52 7.55
Fenpyroximate Content (% w/w) 4.75 to 5.5 5.25 5.11 5.22
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.12 7.10 7.11
Flash point Above 24.5 degree celcius 43 43 43
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies

Room temperature storage data
Parameters Specification
(In house) Study Duration
1 month 6 month 12 month
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.60 30.60 30.59
Clothianidin content (% w/w) 7.125 to 8.25 7.55 7.55 7.53
Fenpyroximate Content (% w/w) 4.75 to 5.5 5.25 5.24 5.22
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.12 7.12 7.11
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies
Flash point Above 24.5 degree celcius 43 43 43

Example 6: Profenofos 30% + Clothianidin 7.5% + Flonicamid 5% EC
Ingredient Percentage (w/w)
Profenofos Technical A.I. 30
Clothianidin Technical A.I. 7.5
FlonicamidTechnical A.I. 5
N-Methyl-2-pyrrolidone 5
Polyaryl phenol ethoxylate (40-70%) & calcium dodecyl benzene solphonate (20-40%) 6
Polyaryl phenol ethoxylate (20-40%) & calcium dodecyl benzene solphonate (40-60%) 4
Trisiloxane Ethoxylate 2
Mixture of heavy aromatic hydrocarbons QS
TOTAL 100.0

Procedure: As per Example 1

Storage stability study
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±20C At 0±20C
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.08 30.01 30.08
Clothianidin content (% w/w) 7.125 to 8.25 7.65 7.59 7.65
FlonicamidContent (% w/w) 4.75 to 5.5 5.15 5.05 5.14
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.07 7.01 7.03
Flash point Above 24.5 degree celcius 43 43 43
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 month
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.08 30.08 30.07
Clothianidin content (% w/w) 7.125 to 8.25 7.65 7.63 7.61
FlonicamidContent (% w/w) 4.75 to 5.5 5.15 5.14 5.10
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.07 7.06 7.04
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies
Flash point Above 24.5 degree celcius 43 43 43

Example 7: Profenofos 30% + Thiamethoxam 7.5% + Fenpyroximate 5% EC
Ingredient Percentage (w/w)
Profenofos Technical A.I. 30
ThiamethoxamTechnical A.I. 7.5
Fenpyroximate Technical A.I. 5
N-Methyl-2-pyrrolidone 5
Polyaryl phenol ethoxylate (40-70%) & calcium dodecyl benzene solphonate (20-40%) 5.9
Polyaryl phenol ethoxylate (20-40%) & calcium dodecyl benzene solphonate (40-60%) 4.1
Trisiloxane Ethoxylate 2
Mixture of heavy aromatic hydrocarbons QS
TOTAL 100.0

Procedure: As per Example 1

Storage stability study
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.47 30.25 30.45
Thiamethoxam content (% w/w) 7.125 to 8.25 7.80 7.55 7.77
Fenpyroximate Content (% w/w) 4.75 to 5.5 5.29 5.12 5.28
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.09 7.05 7.08
Flash point Above 24.5 degree celcius 43 43 43
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 month
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.47 30.45 30.42
Thiamethoxam content (% w/w) 7.125 to 8.25 7.79 7.78 7.69
Fenpyroximate Content (% w/w) 4.75 to 5.5 5.28 5.26 5.21
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.09 7.09 7.08
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies
Flash point Above 24.5 degree celcius 43 43 43

Example 8: Profenofos 30% + Thiamethoxam 7.5% + Flonicamid 5% EC
Ingredient Percentage (w/w)
Profenofos Technical A.I. 30
ThiamethoxamTechnical A.I. 7.5
Flonicamid Technical A.I. 5
N-Methyl-2-pyrrolidone 5
Polyaryl phenol ethoxylate (40-70%) & calcium dodecyl benzene solphonate (20-40%) 5.5
Polyaryl phenol ethoxylate (20-40%) & calcium dodecyl benzene solphonate (40-60%) 4.5
Trisiloxane Ethoxylate 2
Mixture of heavy aromatic hydrocarbons QS
TOTAL 100.0

Procedure: As per Example 1

Storage stability study
Parameters Specification
(In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.58 30.16 30.52
Thiamethoxam content (% w/w) 7.125 to 8.25 7.75 7.45 7.7
Flonicamid Content (% w/w) 4.75 to 5.5 5.25 5.11 5.25
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.05 7.02 7.05
Flash point Above 24.5 degree celcius 43 43 43
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 month
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.57 30.54 30.52
Thiamethoxam content (% w/w) 7.125 to 8.25 7.74 7.72 7.69
Flonicamid Content (% w/w) 4.75 to 5.5 5.24 5.22 5.18
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.05 7.05 7.04
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies
Flash point Above 24.5 degree celcius 43 43 43

Example 9: Profenofos 30% + Imidacloprid 7.5% + bifenthrin 7.5% EC
Ingredient Percentage (w/w)
Profenofos Technical A.I. 30
Imidacloprid Technical A.I. 7.5
Bifenthrin Technical A.I. 7.5
N-Methyl-2-pyrrolidone 5
Polyaryl phenol ethoxylate (40-70%) & calcium dodecyl benzene solphonate (20-40%) 6
Polyaryl phenol ethoxylate (20-40%) & calcium dodecyl benzene solphonate (40-60%) 4
Trisiloxane Ethoxylate 2
Mixture of heavy aromatic hydrocarbons QS
TOTAL 100.0

Procedure: As per Example 1

Storage stability study
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.33 30.16 30.30
Imidacloprid content (% w/w) 7.125 to 8.25 7.60 7.58 7.59
Bifenthrin Content (% w/w) 7.125 to 8.25 7.62 7.51 7.6
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.11 7.05 7.09
Flash point Above 24.5 degree celcius 43 43 43
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 month
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.32 30.3 30.28
Imidacloprid content (% w/w) 7.125 to 8.25 7.60 7.60 7.59
Bifenthrin Content (% w/w) 7.125 to 8.25 7.62 7.62 7.61
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.11 7.1 7.08
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies
Flash point Above 24.5 degree celcius 43 43 43

Example 10: Profenofos 30% + Imidacloprid 7.5% + Fenpyroximate 5% EC
Ingredient Percentage (w/w)
Profenofos Technical A.I. 30
Imidacloprid Technical A.I. 7.5
Fenpyroximate Technical A.I. 5
N-Methyl-2-pyrrolidone 5
Polyaryl phenol ethoxylate (40-70%) & calcium dodecyl benzene solphonate (20-40%) 5.5
Polyaryl phenol ethoxylate (20-40%) & calcium dodecyl benzene solphonate (40-60%) 4.5
Trisiloxane Ethoxylate 2
Mixture of heavy aromatic hydrocarbons QS
TOTAL 100.0

Procedure: As per Example 1

Storage stability study
Parameters Specification
(In house) Initial Stability (for 14 days)
At 54±20C At 0±20C
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 31.05 30.55 31.01
Imidacloprid content (% w/w) 7.125 to 8.25 7.85 7.58 7.8
Fenpyroximate Content (% w/w) 4.75 to 5.5 5.35 5.14 5.32
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.09 7.05 7.09
Flash point Above 24.5 degree celcius 43 43 43
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies

Room temperature storage data
Parameters Specification
(In house) Study Duration
1 month 6 month 12 month
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 31.01 30.95 30.86
Imidacloprid content (% w/w) 7.125 to 8.25 7.82 7.75 7.72
Fenpyroximate Content (% w/w) 4.75 to 5.5 5.34 5.32 5.29
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.09 7.07 7.06
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies
Flash point Above 24.5 degree celcius 43 43 43

Example 11: Profenofos 30% + Imidacloprid 7.5% + Flonicamid 5% EC
Ingredient Percentage (w/w)
Profenofos Technical A.I. 30
Imidacloprid Technical A.I. 7.5
Flonicamid Technical A.I. 5
N-Methyl-2-pyrrolidone 5
Polyaryl phenol ethoxylate (40-70%) & calcium dodecyl benzene solphonate (20-40%) 5.8
Polyaryl phenol ethoxylate (20-40%) & calcium dodecyl benzene solphonate (40-60%) 4.2
Trisiloxane Ethoxylate 2
Mixture of heavy aromatic hydrocarbons QS
TOTAL 100.0

Procedure: As per Example 1

Storage stability study
Parameters Specification (In house) Initial Stability (for 14 days)
At 54±2 0C At 0±2 0C
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.57 30.26 30.49
Imidacloprid content (% w/w) 7.125 to 8.25 7.68 7.52 7.56
Flonicamid Content (% w/w) 4.75 to 5.5 5.24 5.03 5.25
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.06 7.01 7.03
Flash point Above 24.5 degree celcius 43 43 43
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies

Room temperature storage data
Parameters Specification
(In house) Study Duration
1 month 6 month 12 month
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.56 30.15 30.14
Imidacloprid content (% w/w) 7.125 to 8.25 7.68 7.66 7.62
Flonicamid Content (% w/w) 4.75 to 5.5 5.24 5.22 5.20
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.06 7.05 7.03
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies
Flash point Above 24.5 degree celcius 43 43 43

Example 12: Profenofos 30% + Imidacloprid 7.5% + Tolfenpyrad 7.5% EC
Ingredient Percentage (w/w)
Profenofos Technical A.I. 30
ImidaclopridTechnical A.I. 7.5
Tolfenpyrad Technical A.I. 7.5
N-Methyl-2-pyrrolidone 5
Polyaryl phenol ethoxylate (40-70%) & calcium dodecyl benzene solphonate (20-40%) 5.8
Polyaryl phenol ethoxylate (20-40%) & calcium dodecyl benzene solphonate (40-60%) 4.2
Trisiloxan Ethoxylate 2
Mixture of heavy aromatic hydrocarbons QS
TOTAL 100.0

Procedure: As per Example 1

Storage stability study
Parameters Specification
(In house) Initial Stability (for 14 days)
At 54±20C At 0±20C
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.15 30.05 30.16
Imidacloprid content (% w/w) 7.125 to 8.25 7.71 7.52 7.68
Tolfenpyrad Content (% w/w) 7.125 to 8.25 7.65 7.53 7.63
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.08 7.02 7.08
Flash point Above 24.5 degree celcius 43 43 43
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies

Room temperature storage data
Parameters Specification (In house) Study Duration
1 month 6 month 12 month
Description Yellow to amber colour liquid Complies Complies Complies
Profenofos content (% w/w) 28.5 to 31.5 30.15 30.14 30.12
Imidacloprid content (% w/w) 7.125 to 8.25 7.70 7.68 7.65
Tolfenpyrad Content (% w/w) 7.125 to 8.25 7.64 7.63 7.61
Emulsion stability Max 2ml creaming or sediment after 1 hour Complies Complies Complies
pH (5% in DM water) 6.0 - 8.0 7.08 7.07 7.05
Cold test Any separation or creaming max 2 ml after 1 hour Complies Complies Complies
Flash point Above 24.5 degree celcius 43 43 43

Example 13: Profenofos 20% + Clothianidin 5% + Fipronil 3% OD
Ingredient Percentage (w/w)
Profenofos Technical A.I. 20.00
Clothianidin Technical A.I. 5.00
Fipronil Technical A.I. 3.00
N,N Dimethyl decanamide 10.00
Unsaturated fatty alcohol ethoxylates 4.00
Calcium alkyl benzene sulfonate 5.00
2-Pyrrolidinone, 1-ethenylhexadecyl-,homopolymer 3.00
ethoxylated polyaryl alcohol 7.00
Polyamide 3.00
Adjuvant containing trisiloxane ethoxylate 1.00
Rapeseed oil fatty acid methyl ester QS
TOTAL 100.00

Procedure:
Step 1 Charge required quantity of vegetable oil in vessel and add polyvinyl pyrrollidone, mix well for 30 minutes using high shear homogenizer and pass through horizontal bead mill.
Step 2 Add required quantity of Wetting agent, dispersing agent & suspending agents and homogenize the contents for 45 – 60 minutes using high shear homogenizer.
Step 3 Then add technical materials and homogenize for further 30 minutes.
Step 4 Now pass this homogenized material through horizontal bead mill to get required particle size.
Step 5 After completion of grinding cycles sample is sent to QC for A.I. & particle size analysis
Step 6 After approval from QC, material is transferred to storage tank till packing..

Storage stability study
Specification Initial Heat stability study at 54 + 2 0C for 14 days Cold storage stability at 0 + 2 0C for 14 days
Parameters In House
Description Off-white Complies Complies Complies
Profenofos Content 19 to 21 20.41 20.16 20.39
Profenofos Suspensibility Mini 80% 97.55 96.75 97.01
Clothianidin Content 4.75 to 5.5 5.20 5.02 5.19
Clothianidin Suspensibility Mini 80% 95.75 93.52 94.51
Fipronil Content 2.85 to 3.3 3.15 3.05 3.14
Fipronil Suspensibility Mini 80% 98.65 95.04 97.55
pH 5.0-9.0 7.7 7.5 7.3
Particle size D50 <3, D90 <10 2.5, 8.0 2.7, 8.4 2.9, 8.9
Pourability 95 % min 97.2 96.4 97.1
Specific gravity 1.05 – 1.15 1.09 1.09 1.09
Viscosity 350 -900 cps 700 680 690

Room temperature storage data
Parameters Specification In house Study Duration
1 month 6 month 12 month
Description Off-white Complies Complies Complies
Profenofos Content 19 to 21 20.40 20.38 20.35
Profenofos Suspensibility Mini 80% 97.42 97.38 97.05
Clothianidin Content 4.75 to 5.5 5.20 5.19 5.18
Clothianidin Suspensibility Mini 80% 95.55 95.41 95.05
Fipronil Content 2.85 to 3.3 3.14 3.14 3.13
Fipronil Suspensibility Mini 80% 98.05 97.80 97.52
pH 5.0-9.0 7.7 7.7 7.6
Particle size D50 <3, D90 <10 2.5, 8.0 2.5, 8.0 2.6, 8.1
Pourability 95 % min 97.2 97.2 97.1
Specific gravity 1.05 – 1.15 1.09 1.09 1.09
Viscosity 350 -900 cps 700 700 695

Example 14: Profenofos 20% + Thiamethoxam 5% + Fipronil 3% OD
Ingredient Percentage (w/w)
Profenofos Technical A.I. 20.00
Thiamethoxam Technical A.I. 5.00
Fipronil Technical A.I. 3.00
N,N Dimethyl decanamide 10.00
Unsaturated fatty alcohol ethoxylates 4.00
Calcium alkyl benzene sulfonate 5.00
2-Pyrrolidinone, 1-ethenylhexadecyl-,homopolymer 3.00
ethoxylated polyaryl alcohol 7.00
Polyamide 3.00
Adjuvant containing trisiloxane ethoxylate 1.00
Rapeseed oil fatty acid methyl ester QS
TOTAL 100.00

Procedure: As per Example 13

Storage stability study

Parameters Specification
In House Initial Heat stability study at 54 + 20C for 14 days Cold storage stability at 0 + 20C for 14 days

Description Off-white Complies Complies Complies
Profenofos Content 19 to 21 20.35 20.20 20.33
Profenofos Suspensibility Mini 80% 96.50 95.70 96.15
Thiamethoxam Content 4.75 to 5.5 5.10 5.05 5.10
Thiamethoxam Suspensibility Mini 80% 98.65 96.88 97.96
Fipronil Content 2.85 to 3.3 3.07 3.02 3.07
Fipronil Suspensibility Mini 80% 98.65 96.25 97.26
pH 5.0-9.0 7.5 7.3 7.5
Particle size D50 <3, D90 <10 2.5, 8.1 2.6, 8.3 2.7, 8.9
Pourability 95 % min 97.5 96.1 97
Specific gravity 1.05 – 1.15 1.08 1.08 1.08
Viscosity 350 -900 cps 690 680 690

Room temperature storage data
Specification Study Duration

Parameters In house 1 month 6 month 12 month
Description Off-white Complies Complies Complies
Profenofos Content 19 to 21 20.34 20.32 20.29
Profenofos Suspensibility Mini 80% 96.47 96.41 96.26
Thiamethoxam Content 4.75 to 5.5 5.10 5.09 5.08
Thiamethoxam Suspensibility Mini 80% 98.06 97.86 97.81
Fipronil Content 2.85 to 3.3 3.07 3.06 3.05
Fipronil Suspensibility Mini 80% 98.14 97.85 97.63
pH 5.0-9.0 7.5 7.5 7.4
Particle size D50 <3, D90 <10 2.5, 8.1 2.5, 8.1 2.5, 8.1
Pourability 95 % min 97.5 97.5 97.4
Specific gravity 1.05 – 1.15 1.08 1.08 1.08
Viscosity 350 -900 cps 690 690 690

Example 15: Profenofos 20% + Imidacloprid 5% + Fipronil 3% OD
Ingredient Percentage (w/w)
Profenofos Technical A.I. 20.00
Imidacloprid Technical A.I. 5.00
Fipronil Technical A.I. 3.00
N,N Dimethyl decanamide 10.00
Unsaturated fatty alcohol ethoxylates 4.00
Calcium alkyl benzene sulfonate 5.00
2-Pyrrolidinone, 1-ethenylhexadecyl-,homopolymer 3.00
ethoxylated polyaryl alcohol 7.00
Polyamide 3.00
Adjuvant containing trisiloxane ethoxylate 1.00
Rapeseed oil fatty acid methyl ester QS
TOTAL 100.00

Procedure: As per Example 13

Storage stability study
Specification Initial Heat stability study at 54 + 2 0C for 14 days Cold storage stability at 0 + 2 0C for 14 days
Parameters In House
Description Off-white Complies Complies Complies
Profenofos Content 19 to 21 20.50 20.33 20.47
Profenofos Suspensibility Mini 80% 97.58 96.25 97.55
Imidacloprid Content 4.75 to 5.5 5.13 5.06 5.12
Imidacloprid Suspensibility Mini 80% 98.05 96.23 97.85
Fipronil Content 2.85 to 3.3 3.19 3.04 3.18
Fipronil Suspensibility Mini 80% 97.83 96.21 97.8
pH 5.0-9.0 7.4 7.2 7.4
Particle size D50 <3, D90 <10 2.5, 8 2.7, 8.8 2.9, 8.9
Pourability 95 % min 97.3 96.1 97.0
Specific gravity 1.05 – 1.15 1.09 1.09 1.09
Viscosity 350 -900 cps 680 670 690

Room temperature storage data
Specification Study Duration


Parameters In house 1 month 6 month 12 month
Description Off-white Complies Complies Complies
Profenofos Content 19 to 21 20.49 20.47 20.45
Profenofos Suspensibility Mini 80% 97.51 97.49 97.02
Imidacloprid Content 4.75 to 5.5 5.12 5.11 5.09
Imidacloprid Suspensibility Mini 80% 97.56 97.51 97.29
Fipronil Content 2.85 to 3.3 3.19 3.18 3.15
Fipronil Suspensibility Mini 80% 97.52 97.43 97.28
pH 5.0-9.0 7.4 7.4 7.3
Particle size D50 <3, D90 <10 2.5, 8 2.5, 8.1 2.6, 8.3
Pourability 95 % min 97.3 97.3 97.2
Specific gravity 1.05 – 1.15 1.09 1.09 1.09
Viscosity 350 -900 cps 680 680 675

Example 16: Bio efficacy trials
The synergistic pesticide action of the inventive mixtures can be demonstrated by the experiments below. A synergistic effect exists wherever the action of a combination (ready-mix) of active ingredient is greater than the sum of the action of each of the components alone. Therefore a synergistically effective amount or an effective amount of a synergistic composition or combination is an amount that exhibits greater pesticide activity than the sum of the pesticide activities of the individual components. In the field of agriculture, it is often understood that the term “synergy” is as defined by Colby S.R. in an article entitled “ Calculation of the synergistic and antagonistic responses of herbicide combinations” published in the journal Weeds, 1967, 15, p.20-22, incorporated herein by reference in its entirety. The action expected for a given combination of two active components can be calculated as follows:

Colby’s Formula:

To study the synergistic effect of combination of Profenofos, at least one insecticide of neonicotinoid class and at least one more insecticide, various sets of experiments were conducted in crops like cotton and chilly.
Trial 1: Synergism
The synergistic action of Profenofos + Clothianidin + Bifenthrin, Profenofos+Clothianidin + Fipronil, Profenofos + Clothianidin + Flonicamid, Profenofos+Clothianidin + Tolfenpyrad were studied by conducting bio efficacy experiments on cotton crop.

Details of Experiment:
a) Experiment design : Randomized Block Design
b) Replication : Three
c) Treatments : Twenty
d) Plot size : 20 sq. m.
e) Spacing : 100 cm x 45 cm
f) Test Crop & Variety : Cotton (Ankur 151)
g) Time of application : 45 DAS (Days after sowing), as soon as high Thrips
infestation observed.
h) Spray method : Manually operated knap sack sprayer, using 500 liter
per hectare Water volume

Evaluation Method : The observations were recorded by counting the number of thrips per leaf (3 leaves per plant), 5 plants per plot were observed to record the insect population on 5th days after spraying. The percent insect control (mortality) was worked out by below formula:
Number of thrips in treated plot
% Insect Control = 100 - ------------------------------------------------- X 100
Number of thrips in untreated plot

Table 1: Control of Thrips, Thrips tabaci on cotton crop
Treatments details Dose (g or ml/l water) % Thrips mortality
Obs.Value Cal.Value Ratio
Untreated Check water spray only 0.0
Profenofos 50% EC 0.4 24.5
Clothianidin 50% WDG 0.1 16.2
Bifenthrin 10% EC 0.1 20.3
Fipronil 5% SC 0.06 27.6
Flonicamid 50% WG 0.08 12.7
Tolfenpyrad 15% EC 0.1 25.7
Profenofos 50% EC + Clothianidin 50% WDG 0.4+0.1 32.9 36.7 0.90
Profenofos 50% EC + Bifenthrin 10% EC 0.4+0.1 35.2 39.8 0.88
Profenofos 50% EC + Fipronil 5% SC 0.4+0.06 38.6 45.3 0.85
Profenofos 50% EC + Flonicamid 50% WG 0.4+0.08 32.7 34.1 0.96
Profenofos 50% EC + Tolfenpyrad 15% EC 0.4+0.1 38.2 43.9 0.87
Clothianidin 50% WDG + Bifenthrin 10% EC 0.1+0.1 26.4 33.2 0.79
Clothianidin 50% WDG + Fipronil 5% SC 0.1+0.06 34.4 39.3 0.87
Clothianidin 50% WDG + Flonicamid 50% WG 0.1+0.08 20.2 26.8 0.75
Clothianidin 50% WDG + Tolfenpyrad 15% EC 0.1+0.1 34.3 37.7 0.91
Profenofos 50% EC+ Clothianidin 50% WDG+ Bifenthrin 10% EC 0.4+0.1+0.1 95.3 49.6 1.92
Profenofos 50% EC+ Clothianidin 50% WDG+ Fipronil 5% SC 0.4+0.1+0.06 96.2 54.2 1.78
Profenofos 50% EC+ Clothianidin 50% WDG+ Flonicamid 50% WG 0.4+0.1+0.08 92.8 44.8 2.07
Profenofos 50% EC+ Clothianidin 50% WDG+ Tolfenpyrad 15% EC 0.4+0.1+0.1 98.8 53.0 1.86
EC=Emulsifiable Concentrate, WDG=Water Dispersible Granules, SC=Suspension Concentrate, Obs.Value=Observed Value, Cal. Value=Calculated Value, Ratio = Observed Value/Calculated Value

The field trial observation on thrips control shows that all the inventive tank mix combinations of Profenofos + Clothianidin + Bifenthrin, Profenofos + Clothianidin + Fipronil, Profenofos + Clothianidin + Flonicamid, Profenofos + Clothianidin + Tolfenpyrad were found synergistic and provides an excellent control of Thrips compared to their two active ingredients combinations as well as their solo application (prior art combinations).

Trial 2
Another set of experiment was carried out to study the synergistic action of Profenofos+Thiamethoxam+Bifenthrin, Profenofos+Thiamethoxam+Fipronil, Profenofos+Thiamethoxam+Flonicamid, Profenofos+Thiamethoxam+Tolfenpyrad on cotton crop. The experimental details were same as given in Trial 1. The spraying was done when good infestation of Jassid was observed which was coinciding with 60 days of crop sowing. Evaluation method was same as in case of thrips.

Table 2: Control of Jassid, Amrasca biguttula biguttula on cotton crop
Treatments details Dose (g or ml/l water) % Jassid mortality
Obs.Value Cal.Value Ratio
Untreated Check water spray only 0.0
Profenofos 50% EC 0.4 30.7
Thiamethoxam 25% WG 0.1 26.3
Bifenthrin 10% EC 0.1 32.7
Fipronil 5% SC 0.06 24.3
Flonicamid 50% WG 0.08 40.5
Tolfenpyrad 15% EC 0.1 42.7
Profenofos 50% EC + Thiamethoxam 25% WG 0.4+0.1 45.6 48.9 0.93
Profenofos 50% EC + Bifenthrin 10% EC 0.4+0.1 50.3 53.4 0.94
Profenofos 50% EC + Fipronil 5% SC 0.4+0.06 42.6 47.5 0.90
Profenofos 50% EC + Flonicamid 50% WG 0.4+0.08 53.8 58.8 0.92
Profenofos 50% EC + Tolfenpyrad 15% EC 0.4+0.1 57.2 60.3 0.95
Thiamethoxam 25% WG + Bifenthrin 10% EC 0.1+0.1 44.8 50.4 0.89
Thiamethoxam 25% WG + Fipronil 5% SC 0.1+0.06 40.8 44.2 0.92
Thiamethoxam 25% WG + Flonicamid 50% WG 0.1+0.08 52.3 56.1 0.93
Thiamethoxam 25% WG + Tolfenpyrad 15% EC 0.1+0.1 52.4 57.8 0.91
Profenofos 50% EC+ Thiamethoxam 25% WG+ Bifenthrin 10% EC 0.4+0.1+0.1 98.8 65.6 1.51
Profenofos 50% EC+ Thiamethoxam 25% WG+ Fipronil 5% SC 0.4+0.1+0.06 98.2 61.3 1.60
Profenofos 50% EC+ Thiamethoxam 25% WG+ Flonicamid 50% WG 0.4+0.1+0.08 98.4 69.6 1.41
Profenofos 50% EC+ Thiamethoxam 25% WG+ Tolfenpyrad 15% EC 0.4+0.1+0.1 99.2 70.7 1.40

The synergism was clearly evident from field trial observation on Jassid control on cotton crop. All the inventive tank mix combinations of Profenofos+Thiamethoxam+Bifenthrin, Profenofos+Thiamethoxam+Fipronil, Profenofos+Thiamethoxam+Flonicamid, Profenofos+Thiamethoxam+Tolfenpyrad provides an excellent control of Jassid compared to the all prior art combinations.

Trial 3: Field efficacy against Thrips (Scirtothrips dorsalis) on Chilly (Capsicum annum).
Details of Experiment:
a) Experiment design : Randomized Block Design
b) Replication : Three
c) Treatments : Twenty
d) Plot size : 20 sq. m.
e) Spacing : 100 cm x 45 cm
f) Test Crop & Variety : Chilly (Agnirekha)
g) Time of application : 75 DATP (Days after transplanting), as soon as high
Thrips Infestation observed.
h) Spray method : Manually operated knap sack sprayer, using 600 liter
per hectare Water volume

Evaluation Method : The observations were recorded by counting the number of thrips per twig (3 twigs per plant) by shaking the twig on black color paper. Such 5 plants per plot were observed to record the insect population on at Precount (before spraying) and at 1, 3, 7, 10 and 14th days after spraying. The percent insect control (mortality) was worked out by below formula:
Number of thrips in treated plot
% Insect Control = 100 - ------------------------------------------------- X 100
Number of thrips in untreated plot

Table 3: Treatment details
Treatment No. Treatments Details Formulation (per hectare) Gram active ingredient per hectare

1 Profenofos 30%+ Clothianidin 7.5%+ Bifenthrin 7.5% EC 750 ml 225+56.25+56.25
2 Profenofos 30%+ Clothianidin 5%+ Fipronil 3% OD 1125 ml 225+56.25+33.75
3 Profenofos 30%+Clothianidin 7.5%+Flonicamid 5% EC 750 ml 225+56.25+37.50
4 Profenofos 30%+ Clothianidin 7.5%+ Tolfenpyrad 7.5% EC 750 ml 225+56.25+56.25
5 Profenofos 50% EC + Clothianidin 50% WDG (tank mix) 1000 ml+250 g 500+125
6 Profenofos 50% EC + Bifenthrin 10% EC (tank mix) 1000 ml+1000 ml 500+100
7 Profenofos 50% EC + Fipronil 5% SC (tank mix) 1000 ml+750 ml 500+75
8 Profenofos 50% EC + Flonicamid 50% WG (tank mix) 1000 ml+150 g 500+75
9 Profenofos 50% EC + Tolfenpyrad 15% EC (tank mix) 1000 ml+750 ml 500+75
10 Clothianidin 50% WDG + Bifenthrin 10% EC (tank mix) 250g+1000 ml 125+100
11 Clothianidin 50% WDG + Fipronil 5% SC (tank mix) 250g+750 ml 125+75
12 Clothianidin 50% WDG + Flonicamid 50% WG (tank mix) 250g+150 g 125+75
13 Clothianidin 50% WDG + Tolfenpyrad 15% EC (tank mix) 250g+750 ml 125+75
14 Profenofos 50% EC 1000 ml 500
15 Clothianidin 50% WDG 250g 125
16 Bifenthrin 10% EC 1000 ml 100
17 Fipronil 5% SC 750 ml 75
18 Flonicamid 50% WG 150 g 75
19 Tolfenpyrad 15% EC 750 ml 75
20 Untreated Check 0 0

Table 4: Residual control of Thrips on chilly crop.
Treatment No. Precount (Number/ twig) % Insect Control, Thrips Scirtothrips dorsalis
1 DAA 3 DAA 7 DAA 10 DAA 14 DAA
1 17.27 97.28 95.82 91.26 88.64 80.52
2 14.76 98.36 97.18 93.37 90.53 84.27
3 15.19 96.62 95.37 92.08 90.06 81.63
4 16.83 98.72 97.82 95.36 92.53 87.56
5 14.93 88.72 71.28 60.72 48.62 25.63
6 17.47 84.62 73.28 62.46 46.72 30.82
7 16.27 89.57 82.17 72.37 56.27 40.62
8 15.87 90.63 85.27 76.28 62.16 48.36
9 14.67 92.74 90.37 78.62 67.28 52.18
10 18.06 85.27 78.73 67.42 50.48 38.62
11 16.52 90.63 84.28 76.48 62.83 50.37
12 17.27 91.38 88.38 75.62 63.52 52.73
13 17.63 93.28 90.16 78.83 67.58 56.36
14 16.28 70.18 56.72 22.18 0 0
15 15.67 62.73 38.62 18.58 2.84 0
16 17.16 58.28 28.62 10.74 0 0
17 16.86 66.83 36.18 8.83 0 0
18 15.32 58.52 22.64 0 0 0
19 17.32 70.48 52.16 38.28 20.38 8.63
20 16.75 0 0 0 0 0

The efficacy of inventive mixture of Profenofos + Clothianidin + Bifenthrin, Profenofos + Clothianidin + Fipronil, Profenofos + Clothianidin + Flonicamid, Profenofos + Clothianidin + Tolfenpyrad were found synergistic and provides an excellent control of Thrips compared to all the prior art combinations. All the inventive mixtures studied were provides longer residual control of thrips compared to their two active ingredients tank mixes and solo applications at the higher use rate. This will helpful to the farmers to reduce the number of application (sprays) and thereby reducing the cost of plant protection and the active ingredient loading in to the environment.

,CLAIMS:
We claim;
[CLAIM 1]. A pesticidal composition comprising Profenofos, at least one insecticide of neonicotinoid class selected from Clothianidin, Thiamethoxam and Imidacloprid and at least one more insecticide selected from Bifenthrin, Fipronil, Fenpyroximate, Flonicamid and Tolfenpyrad with one or more inactive excipient.

[CLAIM 2]. The pesticidal composition as claimed in claim 1 wherein
A) Profenofos is in range of 0.1-50%;
B) At least one insecticide of neonicotinoid class selected from Clothianidin, Thiamethoxam and Imidacloprid is in range of 0.1-25%;
C) at least one more insecticide selected from Bifenthrin, Fipronil, Fenpyroximate, Flonicamid and Tolfenpyrad is in range of 0.1-25%.

[CLAIM 3]. The pesticidal composition as claimed in claim 1 or 2 wherein most preferred compositions are selected from:
a) Profenofos + Clothianidin + Bifenthrin;
b) Profenofos + Clothianidin + Fipronil;
c) Profenofos + Clothianidin + Fenpyroximate;
d) Profenofos + Clothianidin + Flonicamid;
e) Profenofos + Clothianidin + Tolfenpyrad;
f) Profenofos + Thiamethoxam + Bifenthrin;
g) Profenofos + Thiamethoxam Ethyl+ Fipronil;
h) Profenofos + Thiamethoxam + Fenpyroximate;
i) Profenofos + Thiamethoxam + Flonicamid;
j) Profenofos + Thiamethoxam + Tolfenpyrad;
k) Profenofos + Imidacloprid + Bifenthrin;
l) Profenofos + Imidacloprid + Fipronil;
m) Profenofos + Imidacloprid + Fenpyroximate;
n) Profenofos + Imidacloprid + Flonicamid;
o) Profenofos + Imidacloprid + Tolfenpyrad;

[CLAIM 4]. The pesticidal composition as claimed in claim 1-3, wherein inactive excipients are selected from the group consisting of dispersant, anti-freezing agent, anti-foam agent, wetting agent, suspension aid, anti-microbial agent, thickener, quick coating agent or sticking agents and buffering agent.

[CLAIM 5]. The pesticidal composition as claimed in claim 1-4, wherein the formulations comprises of formulations selected from Emulsifiable concentrate (EC), Emulsion, oil in water (EW), Suspension Concentrate (SC), Oil Dispersion (OD), Water Dispersible Granules (WDG), Wettable Powders (WP), ZC (A mixed formulation of CS and SC), ZE (A mixed heterogeneous formulation of CS and SE), ZW (A mixed heterogeneous formulation CS and EW)..

[CLAIM 6]. The pesticidal composition as claimed in claim 5, wherein the preferable formulations are Emulsifiable concentrate (EC) and Oil Dispersion (OD).

[CLAIM 7]. The pesticidal composition as claimed in claim 6, wherein Emulsifiable concentrate (EC) formulation comprises:
A) Profenofos is in range of 0.1-50%;
B) at least one insecticide of neonicotinoid class selected from Clothianidin, Thiamethoxam and Imidacloprid is in range of 0.1-25%;
C) at least one more insecticide selected from Bifenthrin, Fipronil, Fenpyroximate, Flonicamid and Tolfenpyrad is in range of 0.1-25%.
D) one or more inactive excipients selected from wetting agent, Filler, Absorbent, Emulsifier, Dispersants, Stabilizers, Anti-caking and Free-flow agent.

[CLAIM 8]. The pesticidal composition as claimed in claim 6, wherein Oil Dispersion (OD) comprises:
A) Profenofos is in range of 0.1-50%;
B) at least one insecticide of neonicotinoid class selected from Clothianidin, Thiamethoxam and Imidacloprid is in range of 0.1-25%;
C) at least one more insecticide selected from Bifenthrin, Fipronil, Fenpyroximate, Flonicamid and Tolfenpyrad is in range of 0.1-25%.
D) one or more inactive excipients selected from wetting agent, Filler, Absorbent, Emulsifier, Dispersants, Stabilizers, Anti-caking and Free-flow agent.

[CLAIM 9]. The pesticidal composition as claimed in claim in any of the preceding claims, wherein the said composition is protection of plants, agricultural and horticultural crops like Genetically Modified Organism (GMO) and non GMO Plant of Cotton (Gossypium spp.), Jute (Corchorus oliotorus), Paddy (Oryza sativa), Wheat (Triticum aestavum), Barley (Hordeum vulgare), Maize (Zea mays), Sorghum (Sorghum bicolor), Ragi (Eleusine coracana), Pearl millet (Pennisetum glaucum), Sugarcane (Saccharum officinarum) , Sugarbeet (Beta vulgaris), Soybean (Glycine max), Peanut (Arachis hypogaea), Sunflower (Helianthus annuus) , Mustard (Brassica juncea), Rape seed (Brassica napus), Linseed (Linum usitatissimum), Sesame (Sesamum indicum), Castor (Ricinus communis), Green gram (Vigna radiate), Black gram (Vigna mungo), Chickpea (Cicer aritinum), Cowpea (Vigna unguiculata), Redgram (Cajanus cajan), Frenchbean (Phaseolus vulgaris), Indian bean (Lablab purpureus), Horse gram (Macrotyloma uniflorum), Field pea (Pisum sativum), Cluster bean (Cyamopsis tetragonoloba), Lentils (Lens culinaris), Brinjal (Solanum melongena), Cabbage (Brassica oleracea var. capitata), Cauliflower (Brassica oleracea var. botrytis), Okra (Abelmoschus esculentus) , Onion (Allium cepa L.), Tomato (Solanum lycopersicun) , Potato (Solanum tuberosum) , Sweet potato (Ipomoea batatas), Chilly (Capsicum annum), Garlic (Allium sativum), Cucumber (Cucumis sativus) and Melons (Cucumis melo), Radish (Raphanus sativus), Carrot (Dacus carota subsp. sativus), Turnip (Brassica rapa subsp rapa), Apple (Melus domestica), Banana (Musa spp.), Citrus groups (Citrus spp.), Grape (Vitis vinifera), Guava (Psidium guajava), Litchi (Litchi chinensis), Mango (Mangifera indica), Papaya (Carica papaya), Pineapple (Ananas comosus), Pomegranate (Punica granatum) , Sapota (Manilkara zapota), Tea (Camellia sinensis), Coffea (Coffea Arabica), Turmeric (Curcuma longa), Ginger (Zingiber officinale), Cumin (Cuminum cyminum), Fenugreek (Trigonella foenum-graecum), Fennel (Foeniculum vulgare), Coriander (Coriandrum sativum), Ajwain (Trachyspermum ammi), Psyllium (Plantago ovate), Black Pepper (Piper nigrum), Stevia (Stevia rebaudiana), Safed musli (Chlorophytum tuberosum), Drum stick (Moringa oleifera), Coconut (Coco nucifera), Mentha ( Mentha spp.), Rose (Rosa spp.), Jasmine (Jasminum spp.), Marigold ( Tagetes spp.), Common daisy (Bellis perennis), Dahlia (Dahlia hortnesis).